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采用衍生化步骤和气相色谱-质谱法同时分析不同化学类别的农药。

Simultaneous analysis of pesticides from different chemical classes by using a derivatisation step and gas chromatography-mass spectrometry.

机构信息

Equipe de Physico-Chimie de l'Atmosphère, LMSPC (UMR 7515 CNRS - Université de Strasbourg), 1, rue Blessig, 67084 Strasbourg Cedex, France.

出版信息

J Chromatogr A. 2011 Nov 4;1218(44):8123-9. doi: 10.1016/j.chroma.2011.08.098. Epub 2011 Sep 10.

Abstract

This work presents a new method to analyse simultaneously by GC-MS 31 pesticides from different chemical classes (2,4 D, 2,4 MCPA, alphacypermethrin, bifenthrin, bromoxynil, buprofezin, carbaryl, carbofuran, clopyralid, cyprodinil, deltamethrin dicamba, dichlobenil, dichlorprop, diflufenican, diuron, fenoxaprop, flazasulfuron, fluroxypyr, ioxynil, isoxaben, mecoprop-P, myclobutanil, oryzalin, oxadiazon, picloram, tau-fluvalinate tebuconazole, triclopyr, trifluralin and trinexapac-p-ethyl). This GC-MS method will be applied to the analysis of passive samplers (Tenax(®) tubes and SPME fiber) used for the evaluation of the indoor and outdoor atmospheric contamination by non-agricultural pesticides. The method involves a derivatisation step for thermo-labile or polar pesticides. Different agents were tested and MtBSTFA (N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide), a sylilation agent producing very specific fragments [M-57], was retained. However, diuron could not be derivatised and the isocyanate product was used for identification and quantification. Pesticides which did not need a derivatisation step were not affected by the presence of the derivatisation agent and they could easily be analysed in mixture with derivatised pesticides. The method can be coupled to a thermal-desorption unit or to SPME extraction for a multiresidue analysis of various pesticides in atmospheric samples.

摘要

本工作提出了一种新的方法,用于通过 GC-MS 同时分析 31 种不同化学类别的农药(2,4-D、2,4-MCPA、α-氯氰菊酯、联苯菊酯、溴苯腈、噻嗪酮、甲萘威、克百威、氯吡嘧磺隆、环丙嘧啶、溴氰菊酯、二甲戊灵、二氯苯氧乙酸、二氯丙醚、氟啶胺、二噁唑、苯氧羧酸类、氟唑磺隆、氟吡草腙、碘甲磺隆、异噁唑草酮、甲草胺、灭草烟、莠去津、恶唑酮、哒螨灵、噻酮酸、三氯吡氧乙酸、三氟氯氰菊酯、氟啶脲、苯醚甲环唑、三氯吡氧乙酸丁酯和三氟甲磺隆)。这种 GC-MS 方法将应用于被动采样器(Tenax(®)管和 SPME 纤维)的分析,用于评估非农业用农药的室内和室外大气污染。该方法涉及热不稳定或极性农药的衍生化步骤。测试了不同的试剂,保留了产生非常特异性片段 [M-57] 的硅烷化试剂 MtBSTFA(N-(叔丁基二甲基甲硅烷基)-N-甲基三氟乙酰胺)。然而,无法对除草定进行衍生化,并且使用异氰酸酯产物进行鉴定和定量。不需要衍生化步骤的农药不受衍生化试剂的存在影响,可以很容易地与衍生化农药一起分析混合物。该方法可以与热解吸单元或 SPME 提取相结合,用于大气样品中各种农药的多残留分析。

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